Process for recovering catalyst from catalysis residue



June 26, 1923. 1 1,460,110 I E. v. OWEN PROCESS FOR RECOVERING CATALYST FROM CA' IALYSIS RESIDUE Filed March 5. 1922 2 Sheets-Sheet 1 June 26, 1923. 1 1.460.110

E. V. OWREN PROCESS FOR RECOVBRING CATALYST FROI.CATALY$IS RESIDUE Fil d Ma ch 3, 1922 2 Sheets-Sheet 2 30 tail, reference '35 modified construction of recove STATES PATENT f oF-Ficia ERNEST V. OWEN, OF CHICAGO,

ILLINOIS, AssmNon .ro run noovnn German or CHICAGO, ILLINOIS,- A CORPORATION OF 'ILLINCOISQ PROCESS FOR EECOVERING CATALYST FROM CATALYSIS BESIDUE.

Application flied March 8, 1922. Serial No. 540388.

To cll'whom it may concern:

Be. it known that I, ERNEST V. O-wTm, a citizen of the United States, residing at Chicago, in the, county of 'Cook and btate of Illinois, have invented certain new and useful Improvements in Processes for Recoverin (Jatalyst from Catalysis Residue, of whic the following'is a. specification.

' This invention relates to a process for separatingfiuid substances having different boiling points. The primary object of the invention is to scparatethe constituents of a liquid mixture by contacting said li uid mixture, in a -finely divided state, witi a' heated surface which is maintained at such 7 a temperature as to volatilize one or more of the constituents while the other or others of the constituents remain in a liquid state. While capable of general application, the invention is'designed more particularly for the se aration and recovery of aluminum.

chlori e from heavy "hydrocarbons with which it may be associated, as in aspent or partially spent catalyst. qx In order that the invention may be fully understood, an illustrative. procedure em.- bodyin the same, together with two alternative orms of apparatus employed inpracticiiig the process, will be being had to the accompanying drawings, in which igure 1 is a vertical section through one form of apparatus. so

Figure 2 is a vertical section through a chamber. 3 is a detail view showing-in plan Figure the centrifugal spraying the construction of disc.

-Fifirures 4 and 5 are detail viewsf showing in p an view and side elevation the con-' struction of the scrapers. Referring to Figures 1, 3,. 4 and 5, "1 represents the furnace supplied with fuel, preferably in fluid form, through the medium of the .pipe 2'and receiving. its combustion supporting medium air, through a grating 3, from a flue 4. Within the heatin'gchamher 5 through which products of the combustion pass in reaching, the outlet port '6, is

located a recovery chamber 7 of plate metal,

which is heated by the gases from the furnajce to a temperature t at induces separation ofthe lower boiling constitaients ofthe liquid, for instance, aluminum chloride frefn hydrocarbon, which ditional force to equi ped is violently to project, in finely ing ingredient is described in deinner wall 8" spaced from rising of the has r en i i' i v reason of its spent or partially spent condition resulting from catalytic action in the -l'0(".OV91'yof gasoline. This recovery chamwhich are to be separated, may be brou lit into intimate heating relation with his heating zone, a revolving disc 9 is mounted centrally within the chamber 7, upon "a shaft 10 which is driven through gear wheels 11, by a shaft 12. Disc 9 is equipped with upstandin vanes 13,-. the general direction of whic is radiahaltheugh the exnot form is preferably curved to lend adthe'peripheral delivery .of he action of the disc so sub ivided form, liquid to e separated, and 76 eause'said liquid to impinge in a fine spray against the inner wall'of the heatingzonc 8 whereb the more volatile or lower boilv yolatilized and released into the upper portion of" thechamber 7 while the heavier andhigher boiling ingredient or ingredients pass down into the collectin trough i at the bottom of chem: her 7. he li u' sprayed is delivered ce'ntra-lly upon t e centrifugal disc 9, by ate pipe 15 leading from any suitable. source of. the liquid.

Inorder toprevent the liquid from coking or caking upon the heating surface of the zone 8, the latter is constructedwith an the outer wall 8" to develop a heating bath 8 which will temper the heating effect and prevent the fluid to be, separated from coming into direct contact'with the wall against which, the products of combustion impinge. In order to keep the inner wall 8 of the heating zone up to the desired temperature, the annular wall 8 is suspended in the bath 8 intermediate of these walls '8 and 8", and with l sufficient vertical dimension to cause circulationrof the liquid of the bath by' the portion adjacentto the outer wall 8" under the increased heat absorbed from-the impinging products Of OOmbUStIOIi. and the down \flow o the liquid of the bath on the inner side of said annular wall. As a suitable fluid for the bath 8, I prefer to use lead which assumes a molten state under the temperature at which the process is worked'and which will circulate in the manner described.

, In order to keep the inner impacting surface of the zone 8 free to receive the mixture to be separated, the revolving disc 9 is equipped with scrapers 16 of suitable number, as for instance four as suggested in Figure 3, and these embrace, in their scraping action, the rear of the wall which is impinged against by the mixture being sprayed. As will be seenin Figures 4-and 5, the scrapers 16 are mounted upon the disc 9 with some freedom of radial movement so "that centrifugal force develops intimate scraping contact.

Beneath the disc 9 is a gas chamber 17 which receives superheated fixed hydrocarbon gases through. pipes 18 and discharges said gases through the passageways 19 (see Figure 5) and upward through the spray or veil of finely subdivided mixture which .is being given off from the periphery of the off in the mixture, escape through the overhead pipe 20 into the absorption chamber 21 where they are drawn into the series of concentric nozzles 22 of-the combining apparatus by a' blast of fresh liquid, for instance, absorbent naphtha, at a relatively low temperature, delivered through pipe 23 from a cooler 24 by a pump 25. The compipe 32 to the trolled bined liquid from pipe 23 and now conden'sed vapors from pipe 20, passdownward' into a settling or separation chamber 26 where the combined product separates as at 27 and the surplus condensing liquid remains in an upper stratum 28. The combined product from the stratum 27 may be drawn off through a pipe 29 controlled by valve 30 to a place of use or to a tank for storage, or it may beby-passed through a pipe 31 to the pump 25 and passed through the cooler 24 back to the combining apparatus 22 to take-up more of. the volatile constituents from .the recovery chamber 7 in order to make a richer mixture. The u-ncombined condensing liquid 28 which accumulates in the chamber 26, passes through pump 25 and is returned through cooler- 24 to the combining "apparatus 22 forthe production of more mixture. In order to keep up the supply of condensing liquid in thechamber 26, the pipe 33 is led from some suitable source of liquid, and connected through a valve 34 with the pipe 32, andvalve 34 is conby a float 35 in the chamber 26 so that the supply of the condensing liquid is ke t up to the desired level.

eavy hydrocarbon which settles 'in the trough 14 can be withdrawn through a pipe 36 and disposed of in any desirable manner or for any useful purpose.

According to Figure 2, a plurality of recovery chambers 7 are provided with-centrifugal discs 9 mounted upon a common shaft 10 adapted to be revolved by a pulley 11. By these discs 9", mixture introduced through pipe 15 is repeatedly discharged in thin veils against heating zones 8 containing circulating fluid baths.8 operated in principle like the bath 8 already described in that they are kept at a temperature which volatilizes the constituent or constituents to be set free, but by means of electrical heating grids 1 receiving current through circuit 1 from any suitable source 1 of electricity. The material of the baths 8 supplied through pipe 37 is preferably a high boiling point hydrocarbon oil or ahydrocarbon With a much higher boiling point-than that of any of the ingredients to be volatilized. Between the centrifugal discs 9 are funnels 15 which collect the non-volatilized portion of the mixture from each antecedent disc and deliver the same centrally upon the succeeding disc, with the result that the mixture is treated to a plurality of recovery operations each corresponding in principle .to that described with reference to Figure 1 and thus insuring more complete recovery of the valuable ingredient in the mixture whlch will escape through the pipes 20 and be dealt with as already described in connection with Figure 1.

From the foregoing description it will be seen that the mixture of ingredients to be separated 'by' a volatilization of one or more of such ingredients to the exclusion of another orothers thereof, is forcibly impinged on a hot surface maintained at a temperature above that Which will induce volatiliz ation f of the ingredient or ingredients to be set free, and below the temperatureof volatilization of the ingredient or ingredients to be leftbehind; that in-impinging the mixture against the hot surface; the mixture 'is spread out into a very thin sheath or veil which is greatly attenuated or subdivided so that all parts thereof are brought into efficient heating relation with the hot surface; that for the purpose of superinducing separation. of the ingredients that are at the temperature at which they become volatile, a vehicle of hot gas, of a quality that cannot vitiate the ingredients to be recovered, is caused to pass transversely through the thin veil of rojected mixture and to pass off with the released'volatiles'in a manner to assist their escape; and that the non-volatile in gradient or ingredients of the mixture is constantly removed from the hot surface so as to leave the latter free and unobstructed for the reception of the oncoming charge of fresh mixture.

I claim: 1. The improvement in the art of recoverin g aluminum chloride from hydrocarbon- 2. The improvement inthe art of recover-.

in aluminum chloride from hydrocarbon with which it has combined in the process of' catalyzation, which -consists in impinging the mixture of hydrocarbon and aluminum chloride, while still in a fluid state, against.

a surface maintained at a temperature suffi- 'cient to volatilize the aluminum chloride and low boiling hydrocarbons while permitting hydrocarbon to settle out, and recovering the volatiles thus released.

3; The improvement in the art of recovering aluminum chloride from hydrocarbon with which it has combined in the process of catalyzation, which consists in impinging the mixture of hydrocarbon and aluminum chloride, while still in a .fluid state and in the'form of a finely divided spray, against a surface maintained at a temperature sufficient to volatilize the aluminum chloride while permitting hydrocarbon to settle out,

ment against a surface at a temperature and recovering the volatile thus released.

4. The improvement in the art of separatin aluminum chloride from aluminum chlori e hydrocarbon which consists in delivering the aluminum chloride hydrocarbon into impingement against a surface heated toa temperature that will release the aluminum chloride by sublimation but leave behind heavy hydrocarbon, and recovering thevolatile so released.

5. The improvement in the art of separatin aluminum chloride from the aluminum ch oride hydrocarbon which consists in delivering thealuminum chloride hydrocarbon in'the form of a thin spray into impingement against a" surface heated to a temperature that will release the aluminum chloride by sublimation but leave behind heavy hydrocarbon, and recovering the vola. tile so released.

6. The improvement in the art of separatin aluminum chloride from aluminum chlori e hydrocarbon which consists in delivering the aluminum chloride hydrocarbon into ering the volatile so released.

impingement against a surface heated to a temperature'that will release the-aluminum chloride.- by sublimation but leave behind heavy hydrocarbon, simultaneously passing hot gas inrelation to the aluminum chloride hydrocarbon that will enable it to assist in releasing'the aluminum chloride, and recov- 7. The improvement 1n the art of separat I ing aluminum chloride from aluminum chloride hydrocarbon which consists in deliver- 1 ing the aluminum chloride hydrocarbon into impingement against a surface heated to a temperature that will release the aluminum chloride by sublimation but leave behind heavy hydrocarbon, simultaneously passing through said thin spray of aluminum chloride hydrocarbon, hot gas adapted to assist in releasing the aluminum chloride, and re- H covering the volatile so released.

8. The improvement in the art of recover- .so a

ing aluminum chloride from spent or-partially spent aluminum chloride hydrocarbon catalyst Which consists in delivering said catalyst in the form of a-spray intoimpinge ment against a surface heated to a degree that, during the interim of contact, heats aluminum chlorideand low boiling hydrocarbon to the vapor point, and leaves high boiling hydrocarbon in liquid form, andrecoveri'ng the resultant volatiles.

Y 9. The improvement in the art of regenerating aluminum chloride hydrocarbon which consists in delivering spent or partially spent aluminum chloride hydrocarbon catalyst in the form of a thin spray, into impingesufi'icient to release the aluminum chloride, together with low boiling hydrocarbon, and leave behind heavy hydrocarbon, in the form leased into absorption relation to a light hydrocarbon liquid.

10. The lmprovement 1n the art of regenerating aluminum chloride hydrocarbon which consists .in delivering spent orpar- 'of liquid, and passing the volatiles thus rebon, simultaneously passing through said I.

spray hot hydrocarbon gas, and then collecting the volatilized aluminum chloride, light hydrocarbon and hydrocarbon-gas, and subjecting them to the absorbing action of liquid hydrocarbon.

Si ned at of arch, 1922.

- ERNEST V. OWEN.

Chicago, Illinois, this 1st day 

